Artificial fuel and process of making same



March 5, 1935. N 1,993,517

ARTIFICIAL FUEL AND PROCESS OF MAKING SAME Filed July 29, 1931 llixENTQR2 BY W XFTSQQY Patented Mar. '5, 1935 I TA ES; 1

" m oninabtrtmlsagwe 1,993,517 FUELAND PRocEss oF Max mo SAME' lc asitstifl empstead,

Ap le-autumn 29,1931, Serial'No; 553,741"

. 5 Claims.

' This. invention relates to cellulse compounds such as cellulosenitrate 'and acetate, sometimes called nitro-cellulose and acetocellulosep and particularly to so called solutions of suchcellu- 5. losecompounds,:andmore especially'to a method and means for Qausing hatiSknown assOIid-ification of suchsolutionsw it 1 i Heretoforepvariouskinds of cellulose com-. pounds have; been dissolvedin various menstrua,and then various kinds andmethods have been employed. to solidify thecellulose compound: whereby the menstrua. will" becpntained inaframework :of cellulose, compound thereby pro? ducing what iscommonlycalled solid 'alcoholf; Y; 15 Methods and means heretofore usedinorder to obtain a satisfactorysolid alcohol haveeither required rathercomplicated mechanisms, difficult to keep free from deposits ofsolidified cellulose compound, or havebeensof such a nature that thesolidifying agent introduced; into the, solution could not be easilycontrolled; within ;nar row limits. r A principal object ofthisinvention is the. pro: duction of a means and method for thesolidificartion of a cellulose compoundsolution 'suchthat complicated andcumbersome machinery obviated, together f with the attendantdifiiculties, due to the deposit of solidified cellulose compound upontheoperative parts of the i-interior and exterior of such machines. v A.further object of 7 this invention 1 is ,thefpro duction of a means andmethod for ;the purpose specified which will enable a solidification tobe accomplished by the introductionof a solidifi cation agent which may"be-controlled as to-quantity within quite narrow limits. 1 I A furtherobject of this invention is the productions of a means and method forthe purpose specified which will resultinthe production of a productquite thoroughly homogeneous" and uniform throughout, therebyinsuringfacOnstaLnt uniform burningwithout frequent flaring up and dyingdown. i r 1, A further objectofthis invention is the production of ameans and method for the purpose specified, which will .be inexpensive,-result in the leastamount of waste -by-produot, and vvhich may beusable successfully by persons of slight manipulativeskill. Otherobjects and advantages will appear as the description of the particular.physical e1n bodiments {selected to illustrate the invention.progresses,'and the novel features will,;be particularly pointed out inthe appended claims. W

In describing the invention :in detail and the 'larsolvent which Iintend to use for making'a s (Cl. 44-7) r V particular physicalembodiments selectedjto il lustrate'the invention, reference willbeh'adto; theaccompanying drawing and the characters ofreierencethereon. i V r :The drawing, by. a single figure, illustratesal solid alcohol container with solidified material therein and asolidifyingjmeans made inac-j cordance with my invention is placedtherein In order-to carry out my. invention; I'select a cellulosecompound which is soluble in the partic lution thereof.Nitro-cellulosesf are obtainable which are soluble in commercial methylalcohol The solvent power of the commercial methylgjal cohol. is, as iswell known, duet'o thepresence; therein of acetone. Nitro-cellulosejofanitrogen: content may. be obtained gwhi ch are. soluble anhydrc ausethyl alcohol. 1 When ,a nitrogcellu l lose which .islsolubleinanhydrous ethylflalcohol isvus'ed, thenitro-cellulose after beingdissolved in a small quantity of anhydrousethyl alcohol may then bediluted largely with an' ordinary] ethyl alcohol, which may containfrom'5,.to"1, 0

of water, without coagulatinglor precipitating the dissolvednitro-cellulose. l'he jdilutin'g alcohol may contain in. additiontolwater, a denaturant,

such asmethyl alcohol lorpyridin'e, without cans ing a precipitation ofthe. dissolved nitro-cellulosefg I may use a nitro'ecellulosesolubleinamylace; tate and; after 'the. solution of] nitro-cellulosedilute with ordinary ethyl alcohol in-thesame manner as, abovedescribed, in a caseof, nitroe cellulose; soluble in anhydrous'ethylalcohollf i j I mayalso form a nitro cellulose solution quite comparablewith the ordinary collodionfloi merce, that is, I may dissolve anitro-cellulo any alcohol-ether mixture. The ether ordinarily used in makingordinary pharmaceutical collodion is ethylether, but I may substitute;for 40 that ether, another tether, such as methyl ether,

-orpropyl ether, or use a, mixed or compound ether, such as-methyl-ethyl, or ethyl -propyl ether. i V v .In fact thereare aninnumerable numbergot nitro-cellulose. solvents suitable for useassolvents for a .nitro-cellulose' to be a used, lin accordance withmethod, for-the making, or ,asolid alcohol. .Ihe determiningcharacteristic of'flthe sol "ent to be used resides inthe fact thatthen'tro' (cellulose must be precipitatable thereir means of water,either as 'a'liquid, 011 a so inthe case of'ice, or as a vapor as inthe; case of steam, 5., I i f Instead ofcnitro-cellulose I mayuse'pthjje ,lulosefesters, such as cellulose acetate, orjpre ably, ahydrated sulpho-nitro-cellulose acetate, such as has been described inmy copending application filed on even date herewith Serial No. 553,739.In case I use the hydrated sulpho-nitrocellulose acetate I would preferthe form thereof soluble in cold 95% water diluted pure ethyl alcohol.to the last named base would be a mixture of 95% water diluted ethylalcohol and 95% water diluted commercial methyl alcohol. I

The particular solvent preferred by me, when using nitro-cellulose isanhydrous ethyl alcohol.-

The particular diluent preferred byme is the ordinary pure ethyl alcoholcontaining 'notover, about 5% of water and containing as a denaturant ifnecessary, on account of governmental regula- I tions, methyl alcohol,and preferably free from substances which produce an evil ordisagreeable odor when burned, such as pyridine. I

, Various quantities of nitr c-cellulose soluble in anhydrous ethylalcohol, may be dissolved in anhydrous ethyl alcohol, but formypurposes, I prefer to dissolve approximately 3 pounds of substantiallynitro-cellulose, made anhydrousby al cohol displacement, in 40 poundsof'anhydrous ethyl alcohol either pure or denatured as requi'redbygovernmental regulations. After complete solution, various amounts ofdiluents may be addedtheretoybutI prefer to add to such a solution, asis just above described, approximately 60 pounds of about 95% ethylalcohol, denatured by theaddition of the smallest quantity possible,

in compliance withgovernmental regulations, of

methyl'alcohol. Such a procedure-should give me a nitro-cellulosealcohol solution containing about 3% of intro-cellulose. v

Havingobtained'a suitable nitro-cellulose soluis shown in the drawingand designatedl. v It is of a usual, form, and consists essentially of ahollow cylinder provided with a bottom portlon2,

and an annulus 3 at the top thereof which 1s adapted and constructed toreceive and tightly solution. This solidifyingagent I prefer tointroduce, in such a manner as not to disturb the homogeneity oruniformity of the solution. The

solidifying agent may be poured upon the top of the solution; If wateris used as a solidifying agent, as soon as the water touches thetop'surface of the nitro-cellulose solutionfa solidification will takeplace and the water will remain upon the top of the solution until such.time'as diffusion'has taken place throughout the entire massiwhereby thewater top of the solution will be exchanged for 'alcohol,and perhapssolvent in the solution, until the fluid on top of the solution arrivesat substantially the same percentage composition as the solution" heldwithin the framework or'p'ores of the nitro-cellulose which has Anothersolvent particularly applicable .In order to carry this outsuccessfully, the nitrocellulose solution may be poured upon a sheet ofmaterial impervious to the solution, such as,

moistened cotton placed in the bottom of a pan having a perforatedbottom, then the pan placed in a body of water 'so'that the top edgethereof: is not below the surface of the water. This method may be usedbut its use necessitates the later cutting of the mass into small bodiesadapted for being packed into a container such as 1, so that an extraoperation is required;

In order to obviate the difiiculties of the prior methods described, andin order to obtain a uniform. and homogeneous product, applicant prefersto solidify the nitrocellulose solution in the container in which it isto be dispensed, and

to that end, and in accordance with hisinvention prefer to extend it tosome little height above the nitro-cellulose solution, in order that itmay be grasped by thumb and fingers and withdrawn after thesolidification action has taken lace, Of course, I do not mean by thisdescription to exclude other constructions which do not necessitatecarrying the body 5 to the height specified, and do not intend toexclude specifically suchconstructions as to involve a manipulating member, as a rod, 'imbedded in'the member 5 and protruding from the topthereof which would allow the member 5 'to be of less length and stillbe capable'of manual manipulation in withdrawing the samefrom the bodyof the nitro-cellulose.

In any event, the top of, the member 5 must be such that after themember 5 has been put in place the cover 4 may be'put in place, and thecan with its contents of nitro-cellulose solution and the solidifyingmember 5 may be set aside until such time as the solidification hastaken place.

" As a solidifying body 5, I may use a substance which is sufficientlysolid to substantially retain its form and of sufficient structuralstrength to enable it to be manually handled, and which is characterizedby itsability to contain a solidifying liquid capable'of being diffusedfrom the body to and throughout the mass of nitro-cellulose solution,and abody to which the solidified nitro-cellulose will not adhere afterbeing solidified, so that the body'may be easily withdrawnthere'from.

As a solidifying substance, I prefer the use of water and as a body tocarry the water I prefer a body of soap.

The particular soap preferred'by me for use with my invention is onewhich I make by a method preferred by me. This method consists in takingstearic acid and boiling it with alcohol and water, then after adding afew drops of phenol-phthalein as an indicator, cautiously adding 30degrees Baum caustic soda solution until the stearic acid'and formsodium 'stearate.

entire solution just turns'red, and then allowing the mass to standuntilcold. "When the mass is cold it will be quite hard and firm andmay.

be cut into any desired shaped bodies, such as prisms; Suitableproportions for making this soap are 4 grams of stearic acid, 25 gramsof alcohol, '75 grams of water and sufficient of the designated causticsoda solution to neutralize the Such proportions would give about a 4%soap solution.

Of course, by the specific mentioned of stearic acid, I do not intend toexclude other well known fatty acids which are well known equivalents ofstearic acid.

In order to properly effectuate the solidification which I desire, Itake a plug weighing approximately from 15 to 18 grams made of the solidsoap above described, to about 100 cubic centimeters of nitro-cellulosesolution, that is, the plug 5 would be adjusted in size to corre-.spond, in accordance with the given proportions, with the quantity ofnitro-cellulose solution in the container 1. j i

I prefer to allow the solidifying plug 5 to remain in the closed canfrom 24 to 48 hours. At the expiration of that time, the cover would beremoved, and any liquid at the top of thefsolution would be poured off,the plug removed, and then the cavity left by' the plug filled with anitrocellulose solution corresponding to that originally used, and suchan additional quantity poured into the can or container as will bringthe top of the solution approximately to the line 7, that is, just underthe cover 4, and then the cover 4 would be replacedtightly. Uponstanding, the water in the solidified nitro-cellulose would diiIuse intothe new quantity of unsolidified nitro-cellulose solution added andcompletely solidify it so that the can or container, when it reaches thecustomer, would be completely filled with a solid alcohol. By suitablyadjusting the proportions of the depth of the nitro-cellulose solutionand the diameter of the cylinder 5, I may .very. greatly decrease theaverage distance of any given par ticle of dissolved nitro-cellulosefrom the solidifying agent, water, in the body 5, so that although,

by the solidifying methodby pouring water on the top of thenitro-cellulose solution it is necessary .for the water to travel theentire distance from the top to the bottom of the solution in "order tocompletely solidify it, in'imy method the distance for the water totravel will be so greatly decreased that a much quicker solidificationwill take place. By suitable proportioning, the rapidity of thesolidification may be made almost anything desiredythat is, bysurrounding the body 5 with an extremely thin layerof nitrocellulosesolution, solidification will take place almostimmediately, but as thelayer around the body 5 increases in thickness the solidification willbeto that extent more slow. The preferred speed is a solidification bystanding'over night.-

The moisture'contentof the plug or-body 5 determines the moisturecontent of the solidified nitro-cellulcse and, although I preferamoisture content as specified, nevertheless it is to be understood thatas themoisture content of the plug or body 5 may be varied, so may themoisture content of the solidified nitro-cellulose, and that themoisture content of the plug or body 5, may be controlled within quitenarrow limits. If a liquid collects upon the top of the nitro-cellulosesolution upon standing while being solidified, it

will consist of water and alcohol. poured off if desired.

Although I prefer to remove the'soap plug and This may be cellulose basenevertheless, I may remove the soap plug and put nothing in'its place,or I may leave the plug in place. In case I leave the plug in place, Ido not mean to exclude a shortened plug whereby the cellulose nitratemay be placed over the top thereof.

Although I have particularly described one particular physicalembodiment of my invention, and

explained the principle of the operation thereof,

nevertheless, I desire to have it understood that moisture content, byreason of the control of fill the cavity produced thereby with more ofthe the form selected is merely illustrative, but does not exhaustthepossible physical embodiments of the idea of meansor method underlyingmy invention. V i

What I claim as new and, desire to secureby Letters Patent ofthe UnitedStates, is:

1. The method of solidifying anitro-cellulose I solution which consistsin placing a solid body of solution of 'nitro -cellulose, which consistsin immersing a solid neutral alcoholic sodium stearate containing wamr'therein.

5. The method of solidifying an ethyl alcohol solution of a celluloseester, which consists in immersing a solid neutral alcoholic sodiumstearate containing water therein.

' HERBERT KRANICH.

